Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation technology of citric acid tri-2-propylheptanol ester

A technology of propyl heptyl alcohol ester and tricitric acid, which is applied in the preparation of carboxylic acid esters, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of easy oil production, easy precipitation of products, and large mobility. Achieve the effects of good plasticizing effect, low volatility and high esterification rate

Inactive Publication Date: 2012-08-15
江苏雷蒙新材料有限公司
View PDF3 Cites 6 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because the molecular weight of tributyl citrate (TBC) (360) and the molecular weight of acetyl tri-n-butyl citrate (ATBC) (402) are relatively small, the product is easy to precipitate during use, and the migration is large, and the product is easy to leak. Oil

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Example 1, add 420g (2mol) of citric acid monohydrate, 1264g (8mol) of 2-propylheptanol, catalyst H 2 SO 4 2.1g (0.5% of the mass of citric acid monohydrate), 160g of cyclohexane (approximately 10% of the total mass of reactants) as water-carrying agent, stirred and reacted at 160°C for 2-3 hours, and synthesized citric acid three 2-Propylheptanol ester, treated with 5% Na 2 CO 3 Alkaline solution (addition amount is 40% of the crude product weight of tri-2-propylheptanol citrate) neutralize once, wash twice with water, strip for 2 hours, dry and filter to obtain the finished product tri-2-propylheptanol citrate ester.

[0012] Product test: color <50# (Pt-Co), product saponification value 272.6 mgKOH / g, acid value 0.048 mgKOH / g, moisture 0.022%.

Embodiment 2

[0014] Add 420g (2mol) of anhydrous citric acid, 948g (6mol) of 2-propylheptanol, catalyst H 2 SO 4 , 1.26g (0.3% of the mass of anhydrous citric acid), 140g of cyclohexane (approximately 10% of the total mass of the reactants), stirred and reacted at 150°C for 2-3 hours, and synthesized citric acid three 2 - Propylheptyl ester, treated with 5% Na 2 CO 3 Alkaline solution (addition amount is 50% of the crude product weight of tri-2-propylheptanol citrate) neutralize once, wash twice with water, strip for 2 hours, dry and filter to obtain the finished product tri-2-propylheptanol citrate ester.

[0015] Product test: color <50# (Pt-Co), product saponification value 272.8 mgKOH / g, acid value 0.052 mgKOH / g, moisture 0.025%.

Embodiment 3

[0017] Add 420g (2mol) of citric acid monohydrate, 1896g (12mol) of 2-propylheptanol, catalyst H 2 SO 4 , 4.2g (1% of the mass of citric acid monohydrate), 230g of cyclohexane (approximately 10% of the total mass of the reactant), stirred and reacted at 120°C for 2-3 hours, and synthesized citric acid three 2 - Propylheptyl ester, treated with 8% Na 2 CO 3 Alkaline solution (addition amount is 45% of the crude product weight of tri-2-propylheptanol citrate) neutralize once, wash twice with water, strip for 2 hours, dry and filter to obtain the finished product tri-2-propylheptanol citrate ester.

[0018] Product test: color <50# (Pt-Co), product saponification value 273.2 mgKOH / g, acid value 0.046 mgKOH / g, moisture 0.026%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
Saponification valueaaaaaaaaaa
Acid valueaaaaaaaaaa
Saponification valueaaaaaaaaaa
Login to View More

Abstract

The invention discloses a preparation technology of citric acid tri-2-propylheptanol ester and belongs to the field of a citric acid plasticizer. The preparation technology comprises the following steps: esterifying citric acid monohydrate or anhydrous citric acid and 2-propyl heptanol in the presence of a catalyst H2SO4 to synthetize citric acid tri-2-propylheptanol ester; cyclohexane is used as water-carrying agent in reaction, wherein in the reaction, cyclohexane is used as a water carrying agent, the temperature of the esterification reaction is 120-160 DEG C, the reaction time is 2-3 hours, the molar ratio of citric acid monohydrate or anhydrous citric acid to 2-propyl heptanol is 1: (3-7); neutralizing with a sodium carbonate solution after the esterification reaction is finished; then washing to obtain a citric acid tri-2-propylheptanol ester crude product; and carrying out steam stripping on the crude product to remove excessive 2-propyl heptanol, drying and filtering so as to obtain a tri-2-propylheptanol ester finished product. The technology is high in esterification rate, economic and environment-friendly and suitable for industrial production. The obtained citric acid tri-2-propylheptanol ester has the advantages of non-toxic property, mildew resistance, good plasticizing effect, cold resistance, light fastness, water resistance, small volatility and the like.

Description

technical field [0001] The invention belongs to the technical field of citric acid plasticizers, in particular to a preparation process of tri-2-propylheptyl citrate. Background technique [0002] At present, tributyl citrate (TBC) and acetyl tri-n-butyl citrate (ATBC) are widely used as a new type of plastic plasticizer with good compatibility, high plasticizing efficiency, non-toxicity and strong weather resistance. It has attracted attention and can be used for plasticizing various cellulose resins, as well as food packaging materials and medical and sanitary products. However, because the molecular weight of tributyl citrate (TBC) (360) and the molecular weight of acetyl tri-n-butyl citrate (ATBC) (402) are relatively small, the product is easy to precipitate during use, and the migration is large, and the product is easy to leak. Oil. Contents of the invention [0003] The purpose of this invention is to propose a preparation process for a novel citric acid plastici...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07C69/704C07C67/08C08K5/11
Inventor 曹立军周永芳陈平王志刚
Owner 江苏雷蒙新材料有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com